A Set of Infrared Cells for the Determination of Titanium Oxychloride in Refined Titanium Tetrachloride
SONG Guang-lin1,2, LUO Yun-jun1*, LI Jin-qing1, LI Qing2, TAN Hong2
1. School of Material Science and Engineering, Beijing Institute of Technology, Beijing 100081, China 2. Guizhou Academy of Testing and Analysis, Guiyang 550002, China
Abstract：The content control of the impurities in refined TiCl4 becomes the key part for the quality control of titanium material. Refined TiCl4 is the key procedure in producing titanium sponge. Besides, the content of the impurities in titanium sponge and that of the impurities in refined TiCl4 presents the 4-times enrichment relationship. Therefore, control the content of the oxygen, there is the need to analyze the source of oxygen impurities so that strict control can be conducted over the impurities of refined TiCl4. Determination of TiOCl2 in refined TiCl4 was significant for analysis of its impurities. TiOCl2 could be determined by infrared spectroscopy due to its infrared characteristic spectrum line. However, normal infrared absorption cell was not fit for the sample analysis, because TiCl4 easily reacted with moisture in the air and immediately was hydrolyzed to form highly corrosive hydrochloric acid smoke. According to Lambert-Beer Law, which means the concentration (cx) and absorbance(A)～length (L) curve’s slope have direct ratio. The infrared absorption cell with the window film of ZnSe (10×1 mm, wavenumers: 7 800～440 cm-1) and the glass cell (optical path: 22, 12, 7 and 4 mm) was assembled and utilized in determination of the TiOCl2 in refined TiCl4 by standard addition method. The detection limit of TiOCl2 was 17.8 mg·kg-1, the regression equation was Y=1.011 8X, R=0.996 3; With standard addition method, the regression equation of TiOCl2 was Y=1.940 0X, R=0.997 0, it’s good in linearity relation, the TiOCl2 content in refined TiCl4 is determined to be 833.8 mg·kg-1 and SD up to 40.0 mg·kg-1. RSD of the method precision is between 0.95%～1.94%, while recovery rate is between 88.5%～93.1%. This infrared absorption device was safe, simple and convenient, easily removable and washable, and re-useable. The method could conduct the quantitative analysis over the TiOCl2 content in refined TiCl4 through adding standard sample for one time, it could meet the requirement of determination of TiOCl2 in refined TiCl4.
宋光林1，2，罗运军1*，李晋庆1，李 青2，谭 红2 . 一套红外池测定精四氯化钛中二氯氧钛的含量 [J]. 光谱学与光谱分析, 2015, 35(12): 3427-3430.
SONG Guang-lin1,2, LUO Yun-jun1*, LI Jin-qing1, LI Qing2, TAN Hong2 . A Set of Infrared Cells for the Determination of Titanium Oxychloride in Refined Titanium Tetrachloride . SPECTROSCOPY AND SPECTRAL ANALYSIS, 2015, 35(12): 3427-3430.
